Reacción #161792

ord-7ae36b8265044f15b31fdb65330fa012

Disolventes

Condiciones de reacción

Temperatura
110°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.STIRRINGthe reaction mixture was stirred for a further 10 days at 110° C
  2. 2
    Otroformed
  3. 3
    Filtraciónfiltered
  4. 4
    Otrodried

Procedimiento

Under a nitrogen atmosphere 91 mg (0.61 mmol) sodium-iodide, 6 mg (0.03 mmol) copper iodide and 0.09 mL (0.01 mmol) N,N-dimethylene-ethylene-diamine were added to 0.18 g (0.30 mmol) 3-[5′-bromo-2′-(5-fluoro-2,3-dihydro-indole-1-carbonyl)-3,4,5,6-tetrahydro-2H-[1,4′]bipyridinyl-4-yl]-7-methoxy-1,3,4,5-tetrahydro-benzo[d][1,3]diazepin-2-one in 1.0 mL 1,4-dioxane and the mixture was stirred overnight at 110° C. Then an additional 0.3 mL DMF was added and the reaction mixture was stirred for a further 10 days at 110° C. After being diluted with water the precipitate formed was suction filtered and dried.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08829006B2uspto-grants-2014_09